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以邻氯苯胺和多聚甲醛为反应原料制备MOCA。与以邻氯苯胺和甲醛水溶液为原料的传统工艺相比,用多聚甲醛代替甲醛水溶液,使多聚甲醛在酸催化下慢慢分解生成甲醛,可以保证与邻氯苯胺的反应在比较缓和的条件下进行,避免了大量树脂状物质的生成,提高了产品收率。通过正交试验考察了物料配比、反应时间及反应温度等因素对反应的影响,并确定了最佳的工艺条件为:多聚甲醛与邻氯苯胺摩尔比1∶2,反应时间为3h,反应温度为80℃。最佳工艺条件下产品收率为90.3%。
MOCA was prepared from o-chloroaniline and paraformaldehyde. Compared with the traditional process using o-chloroaniline and formalin as raw materials, paraformaldehyde instead of formalin, the paraformaldehyde slowly decomposes under acid catalysis to form formaldehyde, which can ensure that the reaction with o-chloroaniline is relatively mild Conditions, to avoid the formation of a large number of resinous substances, improve product yield. The effects of material ratio, reaction time and reaction temperature on the reaction were investigated by orthogonal test. The optimum technological conditions were as follows: the molar ratio of paraformaldehyde to o-chloroaniline was 1: 2, the reaction time was 3h, The reaction temperature is 80 ° C. The best yield was 90.3%.